Process for producing confectioners&#39; hard butter



PROCESS FOR PRODUCING CONFECTIONERS HARD BUTTER Alan Roylance,Bebington, England, assignor to Leyer Brothers Company, New York, N.Y.,a corporation of Maine No Drawing. Application December 12, 1957 SerialNo. 702,249

Claims priority, application Great Britain December 21, 1956 14 Claims.(Cl. 99-118) This invention relates to confectioners hard butter, and tothe preparation of fats intended for use as confectioners hard butter.

Confectioners hard butter is employed as an ingredient in themanufacture of sweetstufts, icings, coatings and fillings for biscuits,cakes and other confectionery. Confectioners hard butter is judgedlargely on its ability to melt sharply and completely at bodytemperature and to break sharply and suddenly (snap) at roomtemperature.

It has now been found that certain fractions derived from palm kerneloil by hardening, interesterifying and fractionating are useful asconfectioners hard butter.

According to the present invention there is provided a process for thepreparation of confectioners hard butter from palm kernel oil, whichprocess comprises the steps of hardening the oil to an iodine value ofless than 10, interesterifying the oil, hardening being carried outeither before or after interesterification, and then fractionating thehardened, interesterified oil by means of a solvent, to obtain afraction having a dilatation at 30 C. of not less than 1000 and adilatation at 37 C. of not more than 300.

Preferably, the fraction should have a dilatation at 30 C. of not lessthan 1200, and it is also preferred that the dilatation at 37 C. of thefraction should not be more than 200, more preferably not more than 100.

Mixtures of palm kernel oil with coconut oil may be used as startingmaterials, provided that the coconut oil constitutes not more than 25%,by weight, of the mixture.

. Alternatively, the invention provides a confectioners hard butterwhich comprises a fraction derived from palm kernel oil which oil hasbeen hardened to an iodine value of less than 10 and interesterified,which fraction has a dilatation at 30 C. of not less than 1000 and adilatation at 37 C. of not more than 300.

Hardening may be carried out under conditions of time, temperature andpressure usual in the hardening of oils and fats. Any conventionalcatalyst can be used and frequently it will be convenient to use areduced nickel catalyst. it is preferred to use oils which have beenhardened to an iodine value of less than while, more preferably, fullyhardened oils having an iodine value of less than 1 are used. Generally,it is convenient to carry out the hardening step prior tointeresterifioation, but it is also possible to harden afterinteresterifying.

Interesterification may be carried out under conventional conditions andwill cause a high degree of randomisation of the fatty radicals;preferably substantially complete randomisation is achieved. Suitablecatalysts for interesterifying are the metal alkoxides, such as sodiummethoxide, which may be used in alcoholic, preferably methanolic,solution. Generally, about 0.2% of catalyst, by weight of the oil, issufficient to ensure complete interesterification.

Refining, bleaching and deodorising of the oil may be 2,923,745 PatentedMar. 15, 1960- carried out at any suitable stage. Preferably, bleachinghardening and after interesterifying.

The fractionation of the hardened, interesterified oil may be carriedout by fractional crystallisation from a solvent. Generally, it isadvantageous to carry out the fractionation so as to remove a lowmelting glyceride fraction which may amount, for example in the case ofpalm kernel oil, to as much as 25%, by. weight of the, hardened,interesterified oil, the residual fraction having the characteristicsspecified. Substantially anhydrous acetone is the preferred solvent forfractionation but other substantially anhydrous solvents, for exampleether and light petroleum, may be used. I

To remove the low melting glyceride fraction, it is preferred to carryout the crystallisation using. from 3 to 10 mls. of solvent per gram ofoil. The temperature of crystallisation depends on the conditions used,in particular the ratio of solvent to oil. As a general guide it isusually convenient to use a ratio of solvent to oil of about 4:1(volume/weight) at 20 C. For higher temperatures a lower ratio ofsolvent to oil will usually be necessary. Use of too high a ratio ofsolvent to oil may be disadvantageous as too high a proportion ofglycerides maybe removed, which may lead to a product having anundesirably high dilatation at 37 C. However, a fraction according tothe invention may be obtained from a product having such an undesirablyhigh dilatation at 37 C., by adding oil obtained from the mother liquorsof the crystallisation, for instance, by evaporation, to correct thedilatation and yield a fraction according to the invention.Crystallisations should preferably be left at the crystallisationtemperature until precipitation appears to be complete. The precipitateis then filtered oii, preferably with application of vacuum or pressureand then washed with solvent at a temperature slightly lower than thecrystallisation temperature.

For the determination of dilatations for the purpose of thisspecification, there are used a method and appa: ratus given in SectionCIV, 3e (52) of the D.G.F. Einheitsmethoden published by the DeutscheGesellschaft fiir Fettwissenschaft e.V.

In the melting of fats a characteristic change of volume is observedwhich, especially in the case of fats solid at the normal temperature,manifests itself in a sudden increase in the voltune.

The dilatation or. isothermal melting expansion of a fat is the volumeincrease, which is expressed in mmfi, determined under the conditions ofthe following pro cedure and referred to 25 g., the referencetemperature being given.

The dilatometer is of glass and consists of a vertical graduatedcapillary tube joined at its lower end by a U-shaped capillary tube to aglass bulb surmounted by a neck which is internally ground to take ahollow ground glass stopper. The height (above the lowest point of theU-shaped capillary) of the top of the graduated tube and the top of themouth of the bulb are 350 mm. and 70 mm., respectively. The graduationsextend over a length of 250 to 290 mm, and start 1 cm. from the upperend of the tube. The graduations are marked in intervals of 5 mm.(accurately calibrated), and cover a total volume of 900 mmfi. Theinternal diameter of the bulbis 20 mm. and it has a volume of 7 ml.-(tolerance 10.5 ml.). The internally ground neck of the bulb tapersdownwards from an internal diameter of 15 mm. to an internal diameter of12 mm. and is 26 mm. long. The bulb of the instrument is thus below thelevel of the graduations on the capillary tubing. The stopper to beinserted in the mouth of the bulb is about mm. in length (including theground portion), and is hollow position while a dilatation is beingdetermined.

1.5 ml. of well boiled distilled water containing a little blue ink ispipetted into the bulb of the dilatometer. The dilatometer is thenweighed. A sample of the fat to be examined is thoroughly de-gassed" byheating at.

100" C. under vacuum. The fat (at about 60 C.) is then poured into thebulb of the dilatometer and the ground glass stopper is inserted, carebeing taken not to include any air. The amount of fat added is suchthat, during the determination, the level of water never falls below thelowest of the graduations and never rises above the top of thegraduations. If the initial water level on filling is about two-thirdsof the height of the graduated capillary, these'conditions are usuallyfulfilled. The dilatometer is re-weighed to obtain the weight of fatadded. The hollow stopper is then partly filled with lead shot. It isthen placed in a water bath maintained at 60 C. (i0.1) and a reading ofthe level of the water in the capillary is made. This is the basereadso- The filled dilatometcr is chilled in an ice water bath for 1 /2hours. It is then allowed to warm in an air bath to 26 C. at whichtemperature it is maintained for 40 hours. It is then again chilled inan ice water bath for 1 hours, and then placed in a water bath at 20 C.(:0.1 C.), the dilatometer being immersed to such a depth that the waterlevel is above the middle of the ground glass stopper.

The position of the water meniscus in the capillary is read every halfhour until two successive readings difier by no more than 2 mmfi. Thefinal reading (R is used in the calculations.

A similar procedure is adopted for each temperature I at which thedilatation is required. Thus, R R R and R are successively determined.

Finally the dilatometer is heated again to 60 C. and the base reading isi e-determined. If the initial and final base reading differ by morethan 2 mmfi, the whole operation must be repeated.

THE CALCULATION The value of the dilatation is calculated from thefollowing formula:

I C: t A

The following examples illustrates the invention.

Example 1 250 g. of a sample of refined palm kernel oil of iodine value16.0 was hardened at 180 C. with a conventional nickel/kieselguhrcatalyst equivalent to 0.5% Ni; the iodine value of the hardened oil was4.3,. This oil was twice washedat 90-95 C. with 0.1 N NaGl-i solution,each wash being approximately 25% of the volume of the oil. The oil wasthen transferred to a 1 1. roundbottomed flask and. the extraneouswater, removed by heating for 60 minutes at 9095 C. under a vacuum of15-20mm. Hg. Subsequently the oil was placed in the interesterificationvessel, which is a 500 ml. roundbottOmed flask equipped with means forstirring and passage of. gas through the oil. The actualinteresterification was. preceded by. a. more. intensive drying.treatment in which dry nitrogen was passed through the oil with stir- 7ring at a temperature of 105 Crfor 30 minutes; sodium methoxidecatalyst, equivalent to 0.2% by weight of the oil,-prepared as describedbelow, was then added in the form of a 25% solution inmethanol. Theconditions were maintained for 5 minutes after which the interesterifledoil was transferred to a beaker, cooled to C. and successive waterwashes applied until it was free of catalyst; after drying, the oil wasbleached with an activated bleaching earth and filtered.

g. of the interesterified oil was dissolved in 400 ml. of dry acetoneand the resulting solution cooled and allowed to stand for 16 hours at 0C. The solid fraction was filtered oh" and washed with 100 mLof solventat 0 C.; the solvent-free product (74 g.) had a dilatation of 1170 at 30C. and 95 at 37 C. Subsequently, the final product was deodorised at C.for 3 hours at a pressureof 1-2 mm. Hg.

PREPARATION OF SODIUM METHOXIDE CATALYST Substantially dry methanol wasprepared by the following procedure. 1

24 g. of magnesium and 300 ml. of AR. methanol together with a crystalof iodine were placed in a 1 l. roundbottomed flask fitted with a refluxcondenser. The contents of the flask were gently heated to initiatereaction but once under way it was necessary to cool with ice in orderto keep it under control.

On completion of the reaction the resulting suspen sion of magnesiummethoxide in methanol was refluxed for 2 hours after which the drymethanol was distilled off and used as follows:

220 ml. of the dried methanol were added dropwise via a reflux condenserinto a 1 l. roundhottomed flask containing 23 g. of sodium (cut intosmall pieces about A" square). After complete dissolution of the sodium,the solution was ready for use as an interesterification catalyst.

(The special drying treatment of the methanol may be omitted but theresulting catalyst will be less active.)

Example 2 vfor 16 hours at 0 C. The solid fraction was filtered oif andwashed with 100 ml. of solvent at 0 C; the solvent-free product (66 g.)had a dilatation of 1285 at 30 C. and 250 at 37 C. Subsequently, thefinal product was deodorised at 180 C. for 3 hours at a pressure of 1-2mm. Hg.

I claim:

1. A process for the preparation of confcctioners hard butter from palmkernel oil, which process comprises the steps of hardening the oil to aniodine value of less than 10, randomly interesterifying the oil,hardening and interesterification being carried out in indifferentorder, and then fractionating the hardened, interesterilied oil by meansof a solvent to obtain a 'fraction having a dilatation at30 C. of notless than 1000 and a dilatation at 37 C. of not more than 300.

2. A process according to claim 1 in which the fraction obtained has adilatation at 30 C. of not less than 3. A process according to claim 1in which the. fraction obtained has a dilatation at 37 C. of not morethan 200.

4. A. process according to claim 1 in which the fraction obtained has adilatation at 37 C. of not more than 100.

5. A process according to claim 1 in which the fraction obtained has adilatation at 30 C. of not less than 1200 and a dilatation at 37 C. ofnot more than 200.

6. A process according to claim 1 in which the oil is hardened. to. aniodine. valucof less than 5. v

7. A process according to claim 1 in which the oilis hardened to aniodine value of less than 1.

8. A process for the preparation of confectioners hard butter from palmkernel oil, which process comprises the steps of hardening the oil to aniodine value of less than 5, randomly interesterifying the oil,hardening and interesterification being carried out in indifierentorder, and then fractionating the hardened, interesterified oil by meansof a solvent to obtain a fraction having a dilatation at 30 C. of notless than 1200 and a dilatation at 37 C. of not more than 200.

9. A process according to claim 8 in which the oil is hardened to aniodine value of less than 1.

10. A process according to claim 1 in which the solvent used issubstantially anhydrous acetone.

11. A process according to claim 8 in which the solvent used issubstantially anhydrous acetone.

12. A process according to claim 1 in which the interesterification stepis carried out so as to ensure substantially complete randomisation ofthe fatty radicals.

13. A process according to claim 1 in which the fractionation from asolvent is carried out so as to remove a low melting glyceride fractionof up to 25% by Weight of the hardened, interesterified oil.

14. A process according to claim 1 in which the ratio of solvent tohardened, interesterified oil in the fractionation step is about 4:1volume/weight.

References Cited in the file of this patent UNITED STATES PATENTS2,442,536 Eckcy June 1, 1948 2,657,995 Blum Nov. 3, 1953 FOREIGN PATENTS590,916 Great Britain July 31, 1947

1. A PROCESS FOR THE PREPARATION OF CONFECTIONERS'' HARD BUTTER FROMPALM KERNEL OIL, WHICH PROCESS COMPRISES THE STEPS OF HARDENING THE OILTO AN IODINE VALUE OF LESS THAN 10, RANDOMLY INTERESTERIFYING THE OIL,HARDENING AND INTERESTERIFICATION BEING CARRIED OUT IN INDIFFERENTORDER, AND THEN FRACTIONATING THE HARDENED, INTERESTERIFIED OIL BY MEANSOF A SOLVENT TO OBTAIN A FRACTION HAVING A DILATATION AT 30*C. OF NOTLESS THAN 1000 AND A DILATATION AT 37*C. OF NOT MORE THAN 300.